3-[3-fluoro-4-(trifluoromethyl)phenyl]prop-2-enoic Acid → 3-[3-Fluoro-4-(trifluoromethyl)phenyl]propionic acid

HRID 1844040ノート

反応式

HRID 1844040 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]([OH:16])=[O:15])[CH:5]=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9]>CO.C(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([CH2:12][CH2:13][C:14]([OH:16])=[O:15])[CH:5]=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9]

参加物

4

反応物 1

HCID 27375813-[3-fluoro-4-(trifluoromethyl)phenyl]prop-2-enoic Acid

生成物 1

HCID 467374883-[3-Fluoro-4-(trifluoromethyl)phenyl]propionic acid収率 81.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6212Chloroform溶媒

実験手順

10% NIX was added to a stirred solution of 3-(3-fluoro-4-(trifluoromethyl)phenyl)-acrylic acid (I-77a: 5.5 g, 0.0234 mol) in methanol. The resulting mixture was stirred under hydrogen atmosphere for 4 hours. The reaction was monitored by TLC (5% methanol in CHCl3). The catalyst was filtered through celite bed and the solvent distilled under reduced pressure to afford the crude product. Purification by column chromatography on silica gel (2% methanol in CHCl3) afforded 4.5 g of the product (81.8% yield).

後処理

  1. filtrationThe catalyst was filtered through celite bed
  2. distillationthe solvent distilled under reduced pressure
  3. customto afford the crude product
  4. customPurification by column chromatography on silica gel (2% methanol in CHCl3)

出典と根拠

ORDレコード
ord-952d023f73f04fedab2c6da7a5e6b182
出典データセット
uspto-grants-2015_02
特許番号
US08946260B2

反応ノート

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